EP0466044A1 - Procédé pour préparer des microstructures inorganiques à partir de couches Langmuir-Blodgett - Google Patents

Procédé pour préparer des microstructures inorganiques à partir de couches Langmuir-Blodgett Download PDF

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Publication number
EP0466044A1
EP0466044A1 EP91111208A EP91111208A EP0466044A1 EP 0466044 A1 EP0466044 A1 EP 0466044A1 EP 91111208 A EP91111208 A EP 91111208A EP 91111208 A EP91111208 A EP 91111208A EP 0466044 A1 EP0466044 A1 EP 0466044A1
Authority
EP
European Patent Office
Prior art keywords
layers
inorganic
langmuir
component
organic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP91111208A
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German (de)
English (en)
Inventor
Helmuth Prof. Dr. Möhwald
Petra Tippmann-Krayer
Werner Meisel
Ulrike Höhne
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hoechst AG
Original Assignee
Hoechst AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hoechst AG filed Critical Hoechst AG
Publication of EP0466044A1 publication Critical patent/EP0466044A1/fr
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
    • B05D1/20—Processes for applying liquids or other fluent materials performed by dipping substances to be applied floating on a fluid
    • B05D1/202—Langmuir Blodgett films (LB films)
    • B05D1/208—After-treatment of monomolecular films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Definitions

  • Coated supports are becoming increasingly important in industrial technology.
  • optical waveguide systems or filters for optical purposes are coated with thin films, which due to their low critical surface tension are also suitable for improving the friction properties of these materials, for producing protective layers and for other relevant applications.
  • the production of monomolecular layers and the construction of systems from monomolecular layers of inorganic metals or metal ions is important for the study of surface reactions such as catalysis or corrosion, but in particular also for the construction of magnetic information storage and for optical fields of application.
  • monomolecular layers as subunits for the construction of complex systems. These layers are obtained by transferring monomolecular films from a liquid surface to a suitable solid support. Such films can be easily formed and densely packed on a water surface, for example from molecules of a fatty acid with 20 carbon atoms (arachidic acid, CH3- (CH2) 18-COOH). For this purpose, a solution of the organic acid is dripped onto a water surface that is limited by rigid barriers and a movable raft. The solvent evaporates, and the Remaining molecules are pushed together and packed tightly by a defined force that acts on the raft.
  • a fatty acid with 20 carbon atoms arachidic acid, CH3- (CH2) 18-COOH
  • the molecules have a hydrophilic (eg carboxyl group) and a hydrophobic part (eg hydrocarbon chain) and are very insoluble in water, they are based on the water surface.
  • the hydrophilic groups remain in the water and the hydrophobic chains are erected.
  • the process according to the invention makes it possible to produce inorganic microstructures from Langmuir-Blodgett layers by transferring one or more monomolecular layers of salts of organic acids to a support while maintaining their order and then thermally desorbing the organic component by heating, the metal ion remaining on the support surface .
  • the adjacent layers drawn on the carrier can be made up of the same or different salts as desired.
  • the structure of a layer can be done in the simplest way by the Langmuir-Blodgett method.
  • a layer consisting of several monomolecular layers
  • the organic component of the salt can be, for example, an arachidic acid, stearic acid, palmitic acid or other fatty acid residue, or another amphiphilic acid, for example a charged phospholipid.
  • all metals can be used as the inorganic component, preferably all transition metals, in particular iron, cobalt, cadmium, chromium, copper, nickel, manganese, platinum, silver, gold and rhodium, but also sodium, potassium, calcium, strontium and barium.
  • Polymeric salts can also be used as starting materials.
  • the layers which are suitable for the process according to the invention can be produced by adsorption processes as well as by the Langmuir-Blodgett process.
  • the term “Langmuir-Blodgett layers” is to be understood here to mean generally thin, ideally monomolecular layers or defined multi-layers.
  • the layer structure should be constructed in such a way that the distribution of the metal ions and the organic components alternate along the surface normal.
  • a monolayer of an organic acid is spread on a water surface.
  • the aqueous subphase has a pH greater than 5, preferably in the range from 5 to 9, so that a proton of the organic acid dissociates, the metal ions being removed by adding an inorganic salt (for example chloride, bromide, iodide, nitrate, etc.) are transferred to the subphase.
  • an inorganic salt for example chloride, bromide, iodide, nitrate, etc.
  • the concentration in the subphase is preferably 10 ⁇ 4 to 10 ⁇ 3 M, with trivalent or higher ions the concentration can be many times lower, while with monovalent metals it is above 10 ⁇ 4, preferably above 10 ⁇ 2 M should be.
  • the salt can be placed on a carrier made, for example, of glass or silicon can exist, are transferred, whereby multiple layers are produced by repeated immersion and immersion, in which the layers consisting of the aliphatic chains are intercalated by a metal layer.
  • the method according to the invention can be used to produce microstructures which consist of different metals or metal ions.
  • Subsequent thermal treatment of the multilayer can melt or sublimate it.
  • the organic component is desorbed (at 100 to 350 ° C) while the inorganic component remains on the support surface.
  • the temperatures to be used in each case depend on the corresponding ion and counterion.
  • microstructures with different structures can be produced by the method according to the invention.
  • desorption of iron stearate it was shown that interconnected plate-shaped iron-III-containing solids can be formed which differ from those which are formed by thermal desorption of cadmium arachidate.
  • the diameter of the cadmium clusters is usually in the range from 0.5 to 2 ⁇ m, with a distance of 3 to 5 ⁇ m (example 2). In this case, the clusters formed are not interconnected.
  • the distribution of the microstructures can be controlled by setting preparation parameters such as desorption kinetics, nucleation or layer thickness.
  • the temperatures to be used in the case of thermal desorption depend on the organic and inorganic components used.
  • the bond between the metal and the acid residue must not be too weak, but also not too strong, in order to ensure the desorption and thus the microstructure formation of the metal ions at sufficiently low temperatures.
  • the advantage of the method according to the invention lies in particular in the use of relatively mild temperatures.
  • the method according to the invention allows inorganic microstructures which have a high degree of order to be built up at relatively low temperatures and which can also be laterally structured with the aid of photolithography. Economically interesting aspects would be seen especially in the area of applications in optics, data storage, catalyst technology but also magnetometry.
  • XPS X'ray induced Photoelectron Spectroscopy
  • the measurements were carried out on a cadmium arachidate (FIG. 1a) and an iron (III) stearate (FIG. 1b) multilayer.
  • the coating was carried out using the classic LB technique; Hydrophilic silicon with a natural silicon oxide layer of approx. 20-50 ⁇ was used as the carrier.
  • the cadmium arachidate film consisting of 7 monolayers, was after spreading arachic acid on Millipore water with 10 ⁇ 3 M CdCl2, at pH 7 (6 mg NaHCO3 / 1 water), at 20 ° C and subsequent compression at a constant pressure of 30 mN / m.
  • the iron (III) multilayer stearate (17 monolayers) was formed from stearic acid on a subphase with 4 ⁇ 10 ⁇ 5 M FeCl3, pH 5.5, 40 ° C and at a pressure of 30 mN / m. In both cases the winding speed was 10 mm / min.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Laminated Bodies (AREA)
EP91111208A 1990-07-07 1991-07-05 Procédé pour préparer des microstructures inorganiques à partir de couches Langmuir-Blodgett Withdrawn EP0466044A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4021733A DE4021733A1 (de) 1990-07-07 1990-07-07 Verfahren zur herstellung anorganischer mikrostrukturen aus langmuir-blodgett-schichten
DE4021733 1990-07-07

Publications (1)

Publication Number Publication Date
EP0466044A1 true EP0466044A1 (fr) 1992-01-15

Family

ID=6409896

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91111208A Withdrawn EP0466044A1 (fr) 1990-07-07 1991-07-05 Procédé pour préparer des microstructures inorganiques à partir de couches Langmuir-Blodgett

Country Status (6)

Country Link
EP (1) EP0466044A1 (fr)
JP (1) JPH0592167A (fr)
CA (1) CA2046391A1 (fr)
DE (1) DE4021733A1 (fr)
FI (1) FI913249A7 (fr)
IE (1) IE912355A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0590680A1 (fr) * 1992-10-02 1994-04-06 Matsushita Electric Industrial Co., Ltd. Procédé pour la fabrication de couches organiques
FR2747945A1 (fr) * 1996-04-26 1997-10-31 Lorraine Laminage Traitement de surface de tole metallique

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19928658C2 (de) * 1999-06-23 2002-12-19 Michael Gleiche Verfahren zur Erzeugung geordneter Kanalstrukturen durch Benetzungsinstabilitäten
US8795783B2 (en) * 2009-08-31 2014-08-05 The Regents Of The University Of Michigan Preparation of layer-by-layer materials and coatings from ionic liquids

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4317043A (en) * 1979-10-26 1982-02-23 The University Of Rochester Normal incidence x-ray reflectors and resonant cavities for supporting laser action using the same
EP0359101A2 (fr) * 1988-09-07 1990-03-21 Hoechst Aktiengesellschaft Polyamide et film fabriqué à partir d'une couche au moins monomoléculaire d'un polyamide
DE3936279A1 (de) * 1988-11-02 1990-05-03 Mitsubishi Electric Corp Verfahren zur herstellung eines organischen halbleiterfilms und halbleitervorrichtung mit einem solchen film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4317043A (en) * 1979-10-26 1982-02-23 The University Of Rochester Normal incidence x-ray reflectors and resonant cavities for supporting laser action using the same
EP0359101A2 (fr) * 1988-09-07 1990-03-21 Hoechst Aktiengesellschaft Polyamide et film fabriqué à partir d'une couche au moins monomoléculaire d'un polyamide
DE3936279A1 (de) * 1988-11-02 1990-05-03 Mitsubishi Electric Corp Verfahren zur herstellung eines organischen halbleiterfilms und halbleitervorrichtung mit einem solchen film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DATABASE WPIL, no. 90-175 224,DERWENT PUBLICATIONS LTD, London, GB *
DATABASE WPIL, no. 90-189 605,DERWENT PUBLICATIONS LTD, London, GB *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0590680A1 (fr) * 1992-10-02 1994-04-06 Matsushita Electric Industrial Co., Ltd. Procédé pour la fabrication de couches organiques
US5424098A (en) * 1992-10-02 1995-06-13 Matsushita Electric Industrial Co., Ltd. Method of manufacturing organic films using organic compound and metallic compound
FR2747945A1 (fr) * 1996-04-26 1997-10-31 Lorraine Laminage Traitement de surface de tole metallique
EP0804973A1 (fr) * 1996-04-26 1997-11-05 Sollac S.A. Traitement de surface de tole metallique
US5925417A (en) * 1996-04-26 1999-07-20 Sollac Surface treatment of metal sheet

Also Published As

Publication number Publication date
FI913249L (fi) 1992-01-08
CA2046391A1 (fr) 1992-01-08
FI913249A0 (fi) 1991-07-04
IE912355A1 (en) 1992-01-15
JPH0592167A (ja) 1993-04-16
FI913249A7 (fi) 1992-01-08
DE4021733A1 (de) 1992-01-09

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